Sciencemadness Discussion Board

Please improve this post.

Volitox Ignis - 1-2-2016 at 21:38

I haven't yet asked one of the admins for permission to edit the Wiki,but I think that I might be of some use to the Wiki:

When,and if,I do get access to the Wiki,I want to start a page called "Triethylamine". I haven't fully thought it through yet,but looking through the other pages makes it obvious that a "Preparation" section to a future page is pretty much essential. So unless someone starts the Triethylamine page before me, I ask whoever is reading this to suggest improvements to what I plan to write for "Preparation":

Triethylamine can be prepared by first dissolving equimolar amounts of ethyl bromide and anhydrous ammonia in an excess of absolute ethanol in a suitable container and heating said container in an oven for at least three hours. Then,distill our the alcohol and add hydrochloric acid to the product to convert it to it's salt form. Melt the ethylamine hydrochloride,then filter off the solid ammonium chloride crystals. Then,freebase the ethylamine and add ethyl bromide,then heat in an oven once again and then allow it to cool.

I attached the PDF where I got the synth procedure, I found it while searching "Sciencemadness triethylamine". Will my "simplified" outline yield a reasonable amount of Et3NH2? Should I write anything else for "Preparation"?
Attachment: A MODIFIED METHOD FOR THE PREPARATION OF TRIETHYLAMINE (2).pdf (263kB)
This file has been downloaded 1683 times


[Edited on 2-2-2016 by Volitox Ignis]

crystal grower - 1-2-2016 at 23:43

Hello,
I'm glad there's another one who wants to improve smwiki.
Send U2U to Polverone or Zts16 and they will create account for you;).

Volitox Ignis - 2-2-2016 at 16:31

I have just created the triethylamine page, awaiting feedback.

Marvin - 3-2-2016 at 02:31

Good start on triethylamine. But...


But...


Never simplify the procedure in a primary source. The result is worthless. In this case it has too many words to be a summery and too few to to actually follow. It also has mistakes. Butchering procedures and adapting them to other things is what makes ledgard's books fiction.

Stating the materials used and linking to the method in one line or copying the whole method word for word letter for letter would both work for me.

Volitox Ignis - 3-2-2016 at 15:36

Quote: Originally posted by Marvin  
Good start on triethylamine. But...


But...


Never simplify the procedure in a primary source. The result is worthless. In this case it has too many words to be a summery and too few to to actually follow. It also has mistakes. Butchering procedures and adapting them to other things is what makes ledgard's books fiction.

Stating the materials used and linking to the method in one line or copying the whole method word for word letter for letter would both work for me.

Who is Ledgard? I am going to assume that he's some snake-oil man,only in chemistry.

[Edited on 3-2-2016 by Volitox Ignis]

careysub - 3-2-2016 at 16:27

Quote: Originally posted by Volitox Ignis  

Who is Ledgard? I am going to assume that he's some snake-oil man,only in chemistry.
[Edited on 3-2-2016 by Volitox Ignis]


Yep.
http://www.sciencemadness.org/talk/viewthread.php?tid=64727
http://www.sciencemadness.org/talk/viewthread.php?tid=30854

BTW - the thing that marked the transition from alchemy to chemistry was the adoption by Glauber and others of the practice of writing exact descriptions of procedures followed and their results.

This practice is the fundamental breakthrough that made the emergence of chemistry possible. So the importance of honoring exact descriptions of procedures cannot be over-emphasized.

PHILOU Zrealone - 4-2-2016 at 15:18

"Will my "simplified" outline yield a reasonable amount of Et3NH2?"
Certainly no Et3NH2 but wel some Et-NH2, (Et)2NH , (Eth)3N and also (Eth)4N(+)Br(-)...

Volitox Ignis - 4-2-2016 at 16:12

Quote: Originally posted by PHILOU Zrealone  
"Will my "simplified" outline yield a reasonable amount of Et3NH2?"
Certainly no Et3NH2 but wel some Et-NH2, (Et)2NH , (Eth)3N and also (Eth)4N(+)Br(-)...


I see the mistake that you pointed out now (Blush).


Edit:I followed the threads linked previously and came across a book by Ledgard titled "The Preparatory Manual of Explosives",and decided to see the procedure for preparing TNT (Easier to verify whether it works). The first procedure seems perfectly fine,the rest of the guides on preparing TNT are very questionable though. For example (Preparing TNT from unleaded gasoline):
" Place 920 grams of toluene, 2700 grams of 99% nitric acid, and 3000 grams of premium-unleaded gasoline into a
flask fitted with stirrer and reflux condenser. "

The stoichiometry seems to be off (I would also like to see a flask that can hold over seven liters of liquid (Based on density calculations)),are there any other problems with the TNT portion of the book?




[Edited on 5-2-2016 by Volitox Ignis]

PHILOU Zrealone - 5-2-2016 at 10:41

Quote: Originally posted by Volitox Ignis  

Edit:I followed the threads linked previously and came across a book by Ledgard titled "The Preparatory Manual of Explosives",and decided to see the procedure for preparing TNT (Easier to verify whether it works). The first procedure seems perfectly fine,the rest of the guides on preparing TNT are very questionable though. For example (Preparing TNT from unleaded gasoline):
" Place 920 grams of toluene, 2700 grams of 99% nitric acid, and 3000 grams of premium-unleaded gasoline into a
flask fitted with stirrer and reflux condenser. "

The stoichiometry seems to be off (I would also like to see a flask that can hold over seven liters of liquid (Based on density calculations)),are there any other problems with the TNT portion of the book?
[Edited on 5-2-2016 by Volitox Ignis]

Many processes proposed look fine on paper, but may be hard to do work in practice.

Toluen trinitration with 99% HNO3 should work, but:

-to the expense of a large quantity of HNO3 to circumvent the water produced in the reaction...each NO2 fixed set a H2O free...

-to the expense of a much longer reaction time...69% HNO3 can mononitrate toluen but in organic chembooks it is said not to work because you need NO2(+)...if you get a close look a the interface between toluen and 69% HNO3, you see an immediate yellow colouration (do a search for nitrotoluene under my username in the Energetic material section) but over time (monthes) solid is formed containing most certainly p-nitro-benzoic acid.

-to the expense of byproducts ... oxydation of toluen to benzoic acid derivatives, oxydation of the gasoline (an horrible mix of alcanic hydrocarbons but also of BTEXSN (Benzene, Toluene, Ethylbenzene, Xylenes, Styrene and Naphtalene) as minor ingredients.

This simple example regarded through the prism of chemistry very fast shows the book and writer to be scientifically doubtfull and the text is certainly lacking meaningfull informations to allow things to work the way they are said they should work.

Volitox Ignis - 5-2-2016 at 16:47

Quote: Originally posted by PHILOU Zrealone  
Quote: Originally posted by Volitox Ignis  

Edit:I followed the threads linked previously and came across a book by Ledgard titled "The Preparatory Manual of Explosives",and decided to see the procedure for preparing TNT (Easier to verify whether it works). The first procedure seems perfectly fine,the rest of the guides on preparing TNT are very questionable though. For example (Preparing TNT from unleaded gasoline):
" Place 920 grams of toluene, 2700 grams of 99% nitric acid, and 3000 grams of premium-unleaded gasoline into a
flask fitted with stirrer and reflux condenser. "

The stoichiometry seems to be off (I would also like to see a flask that can hold over seven liters of liquid (Based on density calculations)),are there any other problems with the TNT portion of the book?
[Edited on 5-2-2016 by Volitox Ignis]

Many processes proposed look fine on paper, but may be hard to do work in practice.

Toluen trinitration with 99% HNO3 should work, but:

-to the expense of a large quantity of HNO3 to circumvent the water produced in the reaction...each NO2 fixed set a H2O free...

-to the expense of a much longer reaction time...69% HNO3 can mononitrate toluen but in organic chembooks it is said not to work because you need NO2(+)...if you get a close look a the interface between toluen and 69% HNO3, you see an immediate yellow colouration (do a search for nitrotoluene under my username in the Energetic material section) but over time (monthes) solid is formed containing most certainly p-nitro-benzoic acid.

-to the expense of byproducts ... oxydation of toluen to benzoic acid derivatives, oxydation of the gasoline (an horrible mix of alcanic hydrocarbons but also of BTEXSN (Benzene, Toluene, Ethylbenzene, Xylenes, Styrene and Naphtalene) as minor ingredients.

This simple example regarded through the prism of chemistry very fast shows the book and writer to be scientifically doubtfull and the text is certainly lacking meaningfull informations to allow things to work the way they are said they should work.


I have just created a Wiki page on Ledgard,am I missing anything?

Marvin - 6-2-2016 at 04:51

PH Z is right, but there is another aspect.

Firstly nitrating mixtures can turn oxidising and runaway very rapidly. This produces dense clouds of toxic nitrogen dioxide gas and can throw hot acid everywhere. This quantity may even explode in a real sense. The 'Premium unleaded' in the US specified can contain ethanol, which only increases the chance of an accident.

Secondly some solutions of anhydrous nitric acid in organic solvents can sustain a detonation, so while this may fail to produce any of the expected product that doesn't mean leaving an intact corpse.

ledgard manages to make success much more difficult while making the user much more vulnerable to serious injury and I've had private discussions with people that think his books are deliberate disinformation.

There is a lot more to this, for example he doesn't fix well known mistakes when he releases new editions, and I'm not sure any of it is worth a wiki article beyond "prolific author of some of the least trustworthy fringe material on the internet".

Volitox Ignis - 6-2-2016 at 09:10

Quote: Originally posted by Marvin  

ledgard manages to make success much more difficult while making the user much more vulnerable to serious injury and I've had private discussions with people that think his books are deliberate disinformation.
.


"Deliberate disinformation" sounds about right considering that this "Organic chemist and inventor" has no information available about himself and no patents under his name (Either lying or using a pseudonym,both of which are shady). Just out of curiosity, what did you say to those that thought that Ledgard's work is designed to misinform the reader?

Marvin - 6-2-2016 at 14:36

Mainly that when he was around (roughly turn of the millennium) spamming (mostly unrelated) forums about his books and running his website distributing them he just sounded young. He seemed to think having written the book before going to university made it acceptable to have a load of mistakes. He was also boasting that the US government was going to pay him to distribute it to troops.

Almost certainly a pseudonym. He wrote "King's chemistry survival manual" originally under another name, again probably an alias. Something like John King, a quick google did not get me an answer and I don't feel like chasing.

Mabus - 7-2-2016 at 06:17

Just noticed I added some time ago a reference to one of Ledgard's books in the phosphorus article, and I added a disclaimer, in case the information proves to be false. This also got me thinking:
Should the Ledgard article be expanded to include all the known misinformation from his books? Like what is fact and what is fiction? I think it would be a good idea to have all that info in one place, instead of looking through pages upon pages of discussions.

Marvin - 7-2-2016 at 09:37

Of all the things the wiki could become one of the worst I can think of is a free fact checking service for publishers of fringe literature.

In terms of errors ledgard's work contains a lot of low hanging fruit. Stuff that any person thinking logically should see even without an education in chemistry. Eventually he's going to fix that and when he does it's going to be much harder to point out how bad the core chemistry is.

It's also quite difficult to prove many of those experiments won't work if there isn't an obvious mistake. Even by doing an experiment. Many people here tried to do the magnesium reduction of potassium hydroxide from the patent and failed until Pok succeeded at another forum. One thing I can't tell you is if the TNT synthesis would actually produce any TNT. I can see obvious mistakes and I know how he broke the synthesis he was copying. I can see how much more dangerous it is. But I can't tell you if it would fail to produce any product. Let's say someone tries it, or a variation and lives to produce a yellow product with broad melting range. Is that a success? Who here would be able to test how much MNT, DNT, TNT, DNP, TNP, NB etc. it actually contains?

Talking about it, correcting, legitimises his works. It adds to his cache, and pushes people to fix and attempt his experiments, something *he* *has* *never* *done*. This is akin to listening to someone in your ear saying "This should happen faster add more acid, what's this green stuff? Try adding some".

[soapbox]The internet has brought us face to page with the primary sources and quality secondary and tertiary sources we can navigate with. We don't need to waste time and life on bottom of the barrel partially digested tertiary sources by people with more game than clue. To steal an idiom from Roger Bacon we should close that door such than no man opens it again and open the new such that no man can close it.[/soapbox]

Mabus - 7-2-2016 at 12:09

I was thinking more in the line of "here's why it's [it might be] an obvious mistake", but I see your point.